CN103949461B - A kind of method that uses near-critical water to separate and reclaim the each component material of waste and old circuit board - Google Patents
A kind of method that uses near-critical water to separate and reclaim the each component material of waste and old circuit board Download PDFInfo
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- CN103949461B CN103949461B CN201410174210.2A CN201410174210A CN103949461B CN 103949461 B CN103949461 B CN 103949461B CN 201410174210 A CN201410174210 A CN 201410174210A CN 103949461 B CN103949461 B CN 103949461B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
Abstract
The invention discloses a kind of method that uses near-critical water to separate and reclaim the each component material of waste and old circuit board. Described method is using near-critical water as reaction media, separate and reclaim waste and old circuit board by regulating and controlling temperature, reaction time and interpolation different catalysts, thoroughly separate to reach Copper Foil, glass fabric and resin matrix, the Copper Foil and the glass fabric that wherein reclaim can further directly recycle, resin matrix exists to decompose oily form, main component is phenol and phenol derivatives, can further purify and apply as industrial chemicals. Therefore, this technique has played progradation for the resource of waste and old circuit board, is an environmental friendliness, simple to operate and efficient technology, and its application prospect is boundless.
Description
Technical field
The invention belongs to electron wastes resource and reclaim field, relate to a kind of method that separates and reclaim the each component material of waste and old circuit board.
Background technology
In recent years, along with the fast development of electronics and information industry, electronic product constantly updates, and has produced a large amount of electron wastes. At present, the recycling of WEEE of China is processed in very urgent situation, and not only self produces a large amount of electronic wastes every year, but also meets with the intrusion of external electronic waste. China has become maximum " the electronic waste recycle bin " in the genuine whole world, will hold every year more than 70% electronic waste in the whole world. Some developed country is the processing cost that reduces waste electrical equipment, drive for economic interests, to southeastern coast some areas such as China Guangdong, Zhejiang, a large amount of illegal border crossings shift waste electrical equipment, and the process means with original backwardness is disassembled processing to electron wastes in locality, severe contamination surrounding enviroment, be detrimental to health, social response is very strong.
Existing data shows that in PCBs, metal component accounts for 40%, and resin and plastics account for 30%, and glass fibre accounts for 30%; In discarded PCBs, not only contain a large amount of metals with recovery value as Cu, and also have a certain amount of precious metal as Au, Ag, Pt, Pd etc., their content is more much higher than the grade of general ore, is important secondary resource. At present, waste printed circuit board renewable resources method mainly contains: (1) burning method, although technique is simple, easy to operate and metal recovery rate is high, but the macromolecule organic in old circuit board because of insufficient a large amount of pernicious gases that produce that burn, is conventionally difficult to process and directly enters and in air, produce serious atmosphere pollution in fusion process; (2) mechanical approach, only by relevant plant equipment, old circuit board is pulverized with levigate, reach and recycle the screening installations such as shaking table after enough fineness and isolate metal ingredient wherein, this method energy consumption is high, separate not thorough, macromolecule component does not give recycling, serious waste of resources equally; (3) method of chemical treatment, adopt acid wash to reclaim abandoned printed circuit board, often because economic worth obviously reduces, after causing noble metal to reclaim, the spent acid of discarded object and copper ions is arbitrarily toppled over or is buried, thereby cause serious secondary pollution, although reclaimed precious metal, paid high Environmental costs. Meanwhile, in removal process, can produce acid mist and sour mud, if not its collecting processing also can cause serious secondary pollution. (4) pyrolysismethod is, under the environment of anoxic, abandoned printed circuit board heating (350-900 DEG C conventionally) is made to its decomposition. Utilize pyrolysismethod to reclaim abandoned printed circuit board, can obtain combustible oil gas and metallics, and the waste residue producing in cracking process is as glass fibre etc. also recoverable, therefore, from the angle of discarded object decrement and renewable resources, pyrolysismethod should be a competitive recovery and treatment method. But, circuit board can generate the poisonous and harmful substances such as more shielding smog, simple substance bromine and bromize hydrogen gas in pyrolytic process, these material contaminated environment, and corrosion treatment equipment, and reduced the quality of gained fuel oil.
A kind of hydrothermal treatment consists of disclosing CN102716896A reclaims the method for Copper Foil and glass fibre in discarded circuit board, by wiring board is carried out to hydrothermal treatment consists, make epoxy resin embrittlement in wiring board, lose cementability, thereby make the different component recovery of can fully dissociating.
CN101898197A discloses a kind of method with supercritical fluid recycling waste circuit boards, by supercritical methanol, the resource in discarded circuit board is recycled.
CN102557883A discloses the brominated plastics of a kind of discarded electrical equipment and has transformed in subcritical fluids the method for phenol, to discard brominated plastics and other auxiliary agents processes in fluid is closed in specific Asia, by controlling response parameter, extraction, separation, purifying process, can obtain the plastics of phenol and harmless treatment.
In recent years, along with the development of near critical fluids method processing solid waste, near-critical water is processed recovery and separating waste, worn circuit board becomes an environmental friendliness, simple to operate and efficient technology gradually, has a extensive future.
Summary of the invention
Utilize backward in technique in process, the wasting of resources and the serious present situation of environmental pollution for China's Disposal of Electronic Wastes, the invention provides a kind of method that uses near-critical water to separate and reclaim the each component material of waste and old circuit board. The method is using near-critical water as reaction media, separate and reclaim waste and old circuit board by regulating and controlling temperature, reaction time and interpolation different catalysts, thoroughly separate to reach Copper Foil, glass fabric and resin matrix, the Copper Foil and the glass fabric that wherein reclaim can further directly recycle, resin matrix exists to decompose oily form, main component is phenol and phenol derivatives, can further purify and apply as industrial chemicals. Therefore, this technique has played progradation for the resource of waste and old circuit board, is an environmental friendliness, simple to operate and efficient technology, and its application prospect is boundless.
The object of the invention is to be achieved through the following technical solutions:
Use near-critical water to separate and reclaim a method for the each component material of waste and old circuit board, specifically comprise following step:
(1) pretreatment: the mainboard of waste and old circuit board is dismantled and separated with components and parts, and the components and parts of dismounting are sorted out to rear otherwise processed, and then mainboard is cut into and is of a size of (0.5-2) cm × (0.5-2) cubic block of cm.
(2) near-critical water processing: waste and old circuit board mainboard and 5-20ml water that 1g is sheared join in reactor, then add the catalyst of 0.02g, reactor is airtight, switch on power and start heating, reaction temperature is 280-320 DEG C, after temperature stabilization, start timing, the reaction time maintains 90-150min. Pressure in reactor is by the Pressure gauge monitoring being connected with it, and the pressure in course of reaction in still remains within the scope of 4.5-22.1MPa.
In this step, described catalyst is hydrochloric acid (HCl) and sulfuric acid (H2SO4) etc. acidic materials or NaOH (NaOH) and sodium carbonate (Na2CO3) etc. alkaline matter.
In this step, described waste and old circuit board mainboard and water rate of charge are 1:5 (g/ml), 1:10 (g/ml), 1:15 (g/ml) or 1:20 (g/ml).
(3) extraction of resin matrix catabolite: after near-critical water is processed, powered-down, is cooled to room temperature by reactor taking-up with running water and migrates out reactor product, the water decomposed solution and the solid product that obtain, then be extracted with ethyl acetate water decomposed solution, obtain resin matrix catabolite. Be mainly after testing phenol and phenol derivatives, these phenolic product, through further processing purifying, can be used as industrial chemicals and use, and wherein the content of phenol increases along with the increase in temperature and reaction time. Be scattered in water because brominated flame-retardant is decomposed to form hydrogen bromide (HBr) in near-critical water is processed, therefore the oil-phase product of ethyl acetate extraction does not contain bromo element. In the solid product simultaneously obtaining there is obvious layering in fiber weaving cloth, and Copper Foil is easily peeled off.
(4) recovery of Copper Foil and glass fabric: by the solid product obtaining in step (3) (glass fabric and Copper Foil), soak 20-30h with acetone, then distilled water cleans 3-5 time, be positioned over temperature and be in the baking oven of 95-115 DEG C and dry 2-4h, separate the separated product that just can obtain Copper Foil and glass fabric through simple screening again, and the glass fibre reclaiming is weaved cotton cloth surperficial pure, can directly further use as reinforcing material, the Copper Foil reclaiming is further smelted purifying, can be used as wire, the materials such as copper electrode use.
In the present invention, near-critical water separates the efficiency and the rate of charge that reclaim the each component material of waste and old circuit board, reaction temperature, reaction time and to add the factor such as kind of catalyst closely relevant, each process conditions and parameter determine according to being by behind near-critical water place, make Copper Foil in waste and old circuit board, glass fibre is weaved cotton cloth and can effectively be separated thoroughly with resin matrix three component materials, and obtain respectively its separated product, and then provide convenience for the follow-up recycling of each component material, so course of reaction technological parameter should strictly be controlled, reach best separation and recovering effect.
The difference of the present invention and existing publication is:
(1) this law is bright is processed and can be reached Copper Foil, glass fabric and resin matrix three after waste and old circuit board and separate thoroughly by near-critical water, realize effective separation of the each component material of waste and old circuit board, the solid product obtaining only need to separate the separated product that just can obtain Copper Foil and fiber weaving cloth by simple artificial screening, than separating of Copper Foil in CN102716896A and fiber, the present invention does not need to carry out the subsequent techniques such as fragmentation and sizing screening.
(2) in the present invention, resin matrix can decompose completely, the decomposition liquid product obtaining is mainly phenols and derivative thereof, after being further purified, can be used as industrial chemicals uses, the glass fibre simultaneously reclaiming is weaved cotton cloth surperficial pure, can directly recycle as reinforcing material, and in CN102716896A, resin matrix does not decompose completely, part resin matrix becomes carbon black, affect the separation purity of Copper Foil and fiber, the glass fibre simultaneously obtaining is Powdered, has greatly limited its scope reusing.
(3) in the present invention, system has added acidity or base catalyst, and resin matrix can be realized 100% decomposition at lower temperature, has obviously improved the organic efficiency of the each component material of waste and old circuit board, and has reduced the carbonization degree in decomposition reaction.
Brief description of the drawings
Fig. 1 is that near-critical water separates the flow chart that reclaims the each component material of waste and old circuit board;
Fig. 2 is the GC-MC figure of ethyl acetate extracting resin decomposed solution at differential responses temperature;
Fig. 3 is the digital photograph figure of solid product after near-critical water processing waste and old circuit board;
Fig. 4 is the digital photograph figure of Copper Foil separated product after near-critical water processing waste and old circuit board;
Fig. 5 is the digital photograph figure of glass fabric separated product after near-critical water processing waste and old circuit board;
Fig. 6 is the SEM figure of glass fabric after near-critical water processing waste and old circuit board.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited to this; every technical solution of the present invention is modified or is equal to replacement, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1
As shown in Figure 1, a kind of method that separates and reclaim the each component material of waste and old circuit board with near-critical water, mainly comprise four operations: the separating of extraction, Copper Foil and the fiber weaving cloth of pretreatment, near-critical water processing, resin matrix catabolite, concrete steps are as follows:
(1) pretreatment: the mainboard of waste and old circuit board is dismantled and separated with components and parts, and the components and parts of dismounting are sorted out to rear otherwise processed, and then mainboard is cut into the cubic block that is of a size of 1.0cm × 1.0cm.
(2) near-critical water processing: be that waste and old circuit board mainboard and the 5ml water that 1:5 (g/ml) shears 1g joins in reactor according to rate of charge, then add the hydrochloric acid (HCl) of 0.02g to make catalyst, reactor is airtight, switch on power and start heating, reaction temperature is 300 DEG C, after temperature stabilization, start timing, the reaction time maintains 120min, more than still internal pressure remains on 4.5MPa.
(3) extraction of resin matrix catabolite: after near-critical water is processed, powered-down, reactor taking-up is cooled to room temperature with running water and migrates out reactor product, the water decomposed solution and the solid product that obtain, then be extracted with ethyl acetate water decomposed solution, be mainly after testing phenol and phenol derivatives (as shown in Figure 2), in the solid product simultaneously obtaining there is obvious layering in fiber weaving cloth, and Copper Foil is easily peeled off (as shown in Figure 3)
(4) recovery of Copper Foil and glass fabric: the solid product obtaining in step (3) (glass fabric and Copper Foil) is soaked to 24h with acetone, then distilled water cleans 5 times, be positioned over temperature and be in the baking oven of 100 DEG C and dry 3h, thereby obtain the separated product (as Figure 4-Figure 6) of Copper Foil and glass fabric.
Embodiment 2
Use near-critical water to separate a method that reclaims the each component material of waste and old circuit board, mainly comprise the following step:
(1) pretreatment: the mainboard of waste and old circuit board is dismantled and separated with components and parts, and the components and parts of dismounting are sorted out to rear otherwise processed, and then mainboard is cut into the cubic block that is of a size of 2cm × 2cm.
(2) near-critical water processing: be that waste and old circuit board mainboard and the 15ml water that 1:15 (g/ml) shears 1g joins in reactor according to rate of charge, then add the NaOH (NaOH) of 0.02g, reactor is airtight, switch on power and start heating, reaction temperature is 320 DEG C, after temperature stabilization, start timing, the reaction time maintains 150min. Pressure in reactor is by the Pressure gauge monitoring being connected with it, more than the pressure in course of reaction in still remains on 7.0MPa.
(3) extraction of resin matrix catabolite: after near-critical water is processed, powered-down, reactor taking-up is cooled to room temperature with running water and migrates out reactor product, the water decomposed solution and the solid product that obtain, then be extracted with ethyl acetate water decomposed solution, be mainly after testing phenol and phenol derivatives (as shown in Figure 2), in the solid product simultaneously obtaining there is obvious layering in fiber weaving cloth, and Copper Foil is easily peeled off (as shown in Figure 3).
(4) recovery of Copper Foil and glass fabric: by the solid product obtaining in step (3) (glass fabric and Copper Foil), soak 24h with acetone, then distilled water cleans 5 times, be positioned over temperature and be in the baking oven of 100 DEG C and dry 3h, finally obtain Copper Foil and glass fabric separated product (as Fig. 4,5 and Fig. 6 as shown in).
Embodiment 3
Use near-critical water to separate a method that reclaims the each component material of waste and old circuit board, mainly comprise the following step:
(1) pretreatment: the mainboard of waste and old circuit board is dismantled and separated with components and parts, and the components and parts of dismounting are sorted out to rear otherwise processed, and then mainboard is cut into the cubic block that is of a size of 0.5cm × 0.5cm.
(2) near-critical water processing: be that waste and old circuit board mainboard and the 10ml water that 1:10 (g/ml) shears 1g joins in reactor according to rate of charge, then add the sodium carbonate (Na of 0.02g2CO3) make catalyst, reactor is airtight, switch on power and start heating, reaction temperature is 280 DEG C, starts timing after temperature stabilization, the reaction time maintains 150min. Pressure in reactor is by the Pressure gauge monitoring being connected with it, more than in course of reaction, still internal pressure remains on 5.0MPa.
(3) extraction of resin matrix catabolite: after near-critical water is processed, powered-down, reactor taking-up is cooled to room temperature with running water and migrates out reactor product, the water decomposed solution and the solid product that obtain, then be extracted with ethyl acetate water decomposed solution, be mainly after testing phenol and phenol derivatives (as shown in Figure 2), in the solid product simultaneously obtaining there is obvious layering in fiber weaving cloth, and Copper Foil is easily peeled off (as shown in Figure 3).
(4) recovery of Copper Foil and glass fabric: by the solid product obtaining in step (3) (glass fabric and Copper Foil), soak 24h with acetone, then distilled water cleans 5 times, be positioned over temperature and be in the baking oven of 100 DEG C and dry 3h, finally obtain the separated product (as Figure 4-Figure 6) of Copper Foil and glass fabric.
The invention is not restricted to above-described embodiment, summary of the invention all can be implemented, and has good effect.
Claims (7)
1. use near-critical water to separate and reclaim a method for the each component material of waste and old circuit board, it is characterized in that described method step is as follows:
(1) pretreatment: the mainboard of waste and old circuit board is dismantled and separated with components and parts, mainboard is cut into cubic block;
(2) near-critical water processing: waste and old circuit board mainboard and 5-20ml water that 1g is sheared join in reactor, then add the catalyst of 0.02g, described catalyst is hydrochloric acid, sulfuric acid, NaOH or sodium carbonate, reactor is airtight, switch on power and start heating, reaction temperature is 280-320 DEG C, starts timing after temperature stabilization, reaction time maintains 90-150min, and the pressure in course of reaction in still remains within the scope of 4.5-22.1MPa;
(3) extraction of resin matrix catabolite: after near-critical water is processed, powered-down, is cooled to room temperature by reactor taking-up with running water and migrates out reactor product, the water decomposed solution and the solid product that obtain, then be extracted with ethyl acetate water decomposed solution, obtain resin matrix catabolite;
(4) recovery of Copper Foil and glass fabric: by the solid product obtaining in step (3), soak 20-30h with acetone, then distilled water cleans 3-5 time, be positioned over temperature and be in the baking oven of 95-115 DEG C and dry 2-4h, then separate through simple screening the separated product that obtains Copper Foil and glass fabric.
2. use near-critical water according to claim 1 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that described cubic block is of a size of (0.5-2) cm × (0.5-2) cm.
3. use near-critical water according to claim 2 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that described cubic block is of a size of 1.0cm × 1.0cm.
4. use near-critical water according to claim 2 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that described cubic block is of a size of 2cm × 2cm.
5. use near-critical water according to claim 2 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that described cubic block is of a size of 0.5cm × 0.5cm.
6. use near-critical water according to claim 1 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that described waste and old circuit board mainboard and water rate of charge are 1:5g/ml, 1:10g/ml, 1:15g/ml or 1:20g/ml.
7. use near-critical water according to claim 1 separates and reclaims the method for the each component material of waste and old circuit board, it is characterized in that reaction temperature is 280 DEG C, 300 DEG C or 320 DEG C.
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| CN104384168A (en) * | 2014-09-12 | 2015-03-04 | 中节能六合天融环保科技有限公司 | Treatment method for waste circuit board |
| CN104889140B (en) * | 2015-05-27 | 2017-08-08 | 福建工程学院 | A kind of processing method of waste printed circuit board |
| CN106947109B (en) * | 2017-03-24 | 2020-04-24 | 福建工程学院 | Method for recycling epoxy resin from waste circuit board |
| CN107759826B (en) * | 2017-11-21 | 2020-07-28 | 西安元创化工科技股份有限公司 | Method for degrading thermosetting polyacrylate resin |
| CN109365487B (en) * | 2018-11-30 | 2020-07-07 | 清远市进田企业有限公司 | Efficient energy-saving cleaning process for epoxy coating in waste circuit board |
| CN112679797A (en) * | 2019-10-17 | 2021-04-20 | 中国石油化工股份有限公司 | Method for recovering carbon fiber reinforced resin matrix composite material by subcritical fluid |
| CN113522885B (en) * | 2021-07-09 | 2023-05-09 | 东莞理工学院 | Method for treating waste printed circuit board by near-critical fluid |
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